WO2023109163A1 - Polyurethane gel and preparation method therefor - Google Patents

Polyurethane gel and preparation method therefor Download PDF

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Publication number
WO2023109163A1
WO2023109163A1 PCT/CN2022/113451 CN2022113451W WO2023109163A1 WO 2023109163 A1 WO2023109163 A1 WO 2023109163A1 CN 2022113451 W CN2022113451 W CN 2022113451W WO 2023109163 A1 WO2023109163 A1 WO 2023109163A1
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Prior art keywords
curing agent
thermally conductive
resin
polyurethane gel
agent component
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PCT/CN2022/113451
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French (fr)
Chinese (zh)
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范永江
吉明磊
陈翠萍
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道生天合材料科技(上海)股份有限公司
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Publication of WO2023109163A1 publication Critical patent/WO2023109163A1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • C08L75/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • C08L75/08—Polyurethanes from polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • C08L75/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to the technical field of polyurethane, in particular to a polyurethane gel and a preparation method thereof.
  • Polyurethane is the abbreviation of polyurethane, and its English name is polyurethane. It is an emerging organic polymer material and is known as the "fifth largest plastic". It is widely used in many fields of the national economy because of its excellent performance.
  • the product application fields involve light industry, chemical industry, electronics, textile, medical treatment, construction, building materials, automobile, national defense, aerospace and aviation, etc.
  • polyurethane gel does not contain siloxane components, it has less pollution to the environment and is easy to mix. It is used to replace traditional silicone gel and is a type of gel that is widely used.
  • the Chinese patent with the publication number CN107848285A discloses a polyurethane gel and its manufacturing method.
  • the polyurethane gel has a gel layer and a coating layer covering the gel layer.
  • the gel layer is obtained by at least making the average number of functional groups
  • the coating layer is obtained by reacting an aliphatic polyisocyanate exceeding 2.0 with a polyol having an average functional group number of 3.0 or less, and the coating layer is obtained by at least making aliphatic diisocyanate and/or alicyclic diisocyanate and difunctional active hydrogen It is obtained by reacting the isocyanate and the hydroxyl group in the resin, so that the content of isocyanate can be reduced, so that the hardness of the polyurethane gel is reduced, but when the polyurethane gel is used in electronic components with high heat generation, due to Polyurethane gel has poor heat dissipation effect, and the heat accumulated in polyurethane gel cannot be dissipated quickly, which may easily cause electronic components
  • the purpose of the present invention is to provide a polyurethane gel and its preparation method, which solves the problem that the polyurethane gel cannot dissipate heat quickly, causing the electronic components to be burned out, and at the same time, the hardness of the obtained polyurethane gel is low, which makes the electronic components collide , polyurethane gel can play a cushioning effect.
  • a polyurethane gel according to the present invention includes a thermally conductive curing agent component and a thermally conductive resin component;
  • the thermally conductive curing agent component includes a curing agent component and a first thermally conductive filler
  • the thermally conductive resin component includes a resin component and a second thermally conductive filler
  • the curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the resin component includes a catalyst and a hydroxyl resin;
  • the volume ratio of the thermally conductive curing agent component to the thermally conductive resin component is 1:1.
  • the beneficial effect of the polyurethane gel of the present invention is that: the curing agent component is obtained through the prepolymerization reaction of the hydroxyl resin and the isocyanate chain extender, so that the isocyanate in the curing agent component content is reduced, so that the hardness of the polyurethane gel is lower; the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, the thermally conductive resin component includes a resin component and a thermally conductive filler, and the curing agent The component and the resin component are respectively added with thermally conductive fillers, so that the polyurethane gel has a good thermal conductivity effect, thereby solving the problem that the polyurethane gel cannot dissipate heat quickly and cause the electronic components to be burned out. At the same time, the hardness of the polyurethane gel obtained is Low, so that when the electronic components collide, the polyurethane gel can play a cushioning effect.
  • the content of the curing agent component is 8% to 20%, and the content of the first thermally conductive filler is 80% to 92%.
  • the content of the resin component is 3%-19%, and the content of the second thermally conductive filler is 81%-97%.
  • the content of the hydroxyl resin in the curing agent component is 60% to 90%, and the content of the isocyanate chain extender is 10%. ⁇ 40%.
  • the content of the catalyst is 0.1%-1%, and the content of the hydroxyl resin in the resin component is 99%-99.9%.
  • the isocyanate chain extender is any one of diphenylmethane diisocyanate, isophorone diisocyanate, polyisocyanate and hexamethylene diisocyanate.
  • the hydroxyl resin in the curing agent component and the hydroxyl resin in the resin component are polyether polyol, polyester polyol, castor oil, modified castor oil and sorbitol any of the.
  • the thermal conductivity of the polyurethane gel is 1.5W/mK ⁇ 3.0W/mK.
  • the beneficial effect is that the polyurethane gel can quickly dissipate heat, thereby preventing electronic components from being burned out.
  • the catalyst is any one of dibutyltin dilaurate catalyst, amine catalyst and organozinc catalyst.
  • the beneficial effect is that by adding the catalyst, the heat-conducting curing agent component and the heat-conducting resin component can react more completely, and the reaction time is shortened.
  • the amine catalyst is any one of aliphatic amine catalysts, alicyclic amine catalysts, alcohol compound catalysts and aromatic amine catalysts.
  • Another object of the present invention is to provide a kind of preparation method of polyurethane gel, comprises the following steps:
  • the heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1.
  • the beneficial effect of the preparation method of the polyurethane gel of the present invention is that: the curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the hydroxyl resin and the isocyanate chain extender are prepolymerized to obtain The curing agent component reduces the content of the isocyanate in the curing agent component, thereby making the hardness of the polyurethane gel lower; the thermally conductive resin component includes a catalyst, which can accelerate the subsequent heat conduction The reaction of the resin component and the thermally conductive curing agent component, thereby shortening the reaction time; the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, and the thermally conductive resin component includes a resin component and a thermally conductive filler, so The above-mentioned curing agent component and the above-mentioned resin component are respectively added with thermally conductive fillers, so that the polyurethane gel has a good thermal conductivity effect, thus solving the problem that the
  • the step of using a hydroxyl resin to react with an isocyanate chain extender to prepare a curing agent component includes: after uniformly mixing the hydroxyl resin and the isocyanate chain extender, performing a temperature-raising stirring reaction to Prepare the curing agent component.
  • the temperature of the heating and stirring reaction is 25° C. to 120° C.
  • the time of the heating and stirring reaction is 30 minutes to 6 hours.
  • a polyurethane gel including a thermally conductive curing agent component and a thermally conductive resin component;
  • the thermally conductive curing agent component includes a curing agent component and a first thermally conductive filler
  • the thermally conductive resin component includes a resin component and a second thermally conductive filler
  • the curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the resin component includes a catalyst and a hydroxyl resin;
  • the volume ratio of the thermally conductive curing agent component to the thermally conductive resin component is 1:1.
  • the curing agent component is obtained by performing a prepolymerization reaction with the hydroxyl resin and the isocyanate chain extender, so that the content of the isocyanate in the curing agent component is reduced, thereby making the polyurethane gel
  • the hardness is low;
  • the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler
  • the thermally conductive resin component includes a resin component and a thermally conductive filler, and the curing agent component and the resin component are respectively added with a thermally conductive filler , so that the polyurethane gel has a good heat conduction effect, thereby solving the problem that the polyurethane gel cannot dissipate heat quickly, causing the electronic components to be burned out.
  • the obtained polyurethane gel has a low hardness, so that when the electronic components collide Glue can play a cushioning effect.
  • the content of the curing agent component is 8% to 20%, and the content of the first thermally conductive filler is 80% to 92%. %.
  • the content of the resin component is 3%-19%, and the content of the second thermally conductive filler is 81%-97%.
  • the content of the hydroxyl resin in the curing agent component is 60% to 90%, and the content of the isocyanate chain extender is The content is 10% to 40%.
  • the content of the catalyst is 0.1% to 1%, and the content of the hydroxyl resin in the resin component is 99% to 99.9% %.
  • the isocyanate chain extender is any one of diphenylmethane diisocyanate, isophorone diisocyanate, polyisocyanate and hexamethylene diisocyanate.
  • the hydroxyl resin in the curing agent component and the hydroxyl resin in the resin component are polyether polyol, polyester polyol, castor oil, modified castor Either of sesame oil and sorbitol.
  • the thermal conductivity of the polyurethane gel is 1.5W/mK ⁇ 3.0W/mK.
  • the polyurethane gel can quickly dissipate heat, thereby preventing electronic components from being burned out.
  • the catalyst is any one of dibutyltin dilaurate catalyst, amine catalyst and organozinc catalyst.
  • the amine catalyst is any one of aliphatic amine catalysts, alicyclic amine catalysts, alcohol compound catalysts and aromatic amine catalysts.
  • the aliphatic amine catalyst is N,N-dimethylcyclohexylamine, bis(2-dimethylaminoethyl)ether, N,N,N',N'- Any one of tetramethylalkylenediamine, triethylamine and N,N-dimethylbenzylamine.
  • the cycloaliphatic amine catalyst is solid amine, N-ethylmorpholine, N,N-dimethylformamide (NMM) and N,N'-diethylpiper any of the oxazines.
  • the alcohol compound catalyst is any one of triethanolamine and dimethylethanolamine (DMEA).
  • the aromatic amine catalyst is any one of pyridine and N,N'-lutidine.
  • the catalyst is N,N-dimethylcyclohexylamine, bis(2-dimethylaminoethyl)ether, N,N,N',N'-tetramethylethylene Alkyldiamine, triethylamine, N,N-dimethylbenzylamine, solid amine, N-ethylmorpholine, N,N-dimethylformamide (NMM), N,N'-diethyl Any one of piperazine, triethanolamine, dimethylethanolamine (DMEA), pyridine and N,N'-lutidine.
  • a kind of preparation method of polyurethane gel comprising the following steps:
  • the heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1.
  • the curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the curing agent component is obtained by performing a prepolymerization reaction between the hydroxyl resin and the isocyanate chain extender, so that in the curing agent component The content of the isocyanate is reduced, so that the hardness of the polyurethane gel is lower;
  • the thermally conductive resin component includes a catalyst, which can accelerate the subsequent reaction of the thermally conductive resin component and the thermally conductive curing agent component, thereby Shorten the reaction time;
  • the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, the thermally conductive resin component includes a resin component and a thermally conductive filler, and the curing agent component
  • the step of using a hydroxyl resin to react with an isocyanate chain extender to prepare a curing agent component includes: after uniformly mixing the hydroxyl resin and the isocyanate chain extender, performing The temperature is raised and the reaction is stirred to obtain the curing agent component.
  • the temperature of the heating and stirring reaction is 25° C. to 120° C., and the time of the heating and stirring reaction is 30 minutes to 6 hours.
  • the thermally conductive filler includes thermally conductive powder and a coupling agent.
  • the thermally conductive powder includes at least one of aluminum hydroxide, aluminum oxide, boron nitride and aluminum nitride.
  • the preparation method of the thermally conductive filler includes the following steps:
  • Examples 1-8 and comparative examples of the present invention respectively provide a polyurethane gel, and its specific composition and content are shown in Table 1.
  • the difference between Examples 1-8 and Comparative Example is that the components in the polyurethane gel in Examples 1-8 include thermally conductive fillers, and the components in the polyurethane gel in Comparative Examples do not include thermally conductive fillers.
  • the heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1.
  • the preparation method of comparative example is as follows:
  • the curing agent component is used to react with the resin component to prepare the polyurethane gel, and the volume ratio of the curing agent component to the resin component is 1:1.
  • Thermal conductivity was tested using the test method in standard ASTM D5470; hardness was tested using the test method in standard ASTM D2240.
  • the thermal conductivity of the polyurethane gel in the present invention is 2.0W/mK ⁇ 2.3W/mK, while the thermal conductivity of the polyurethane gel in the comparative example is 0.3W/mK, the thermal conductivity of the polyurethane gel in the present invention
  • the coefficient is far greater than the thermal conductivity of the polyurethane gel in the comparative example;
  • the hardness of the polyurethane gel in the present invention is 0056 degree to 0075 degree, and the hardness of the polyurethane gel in the comparative example is 0020 degree, and the hardness of the polyurethane gel in the present invention is much larger
  • the cushioning effect of the polyurethane gel in the comparative example is better than that of the polyurethane gel in the present invention, but the polyurethane gel of the present invention also meets the market's requirements for hardness.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

The present invention provides polyurethane gel, comprising a heat-conducting curing agent component and a heat-conducting resin component. The heat-conducting curing agent component comprises a curing agent component and a first heat-conducting filler; the heat-conducting resin component comprises a resin component and a second heat-conducting filler; the curing agent component comprises hydroxyl resin and an isocyanate chain extender; the resin component comprises a catalyst and hydroxyl resin; the volume ratio of the heat-conducting curing agent component to the heat-conducting resin component is 1: 1. The problem that an electronic component is burnt out due to the fact that heat of polyurethane gel cannot be quickly dissipated is solved, and moreover, the hardness of the obtained polyurethane gel is low, so that when the electronic component collides, the polyurethane gel can play a buffering effect. The present invention also provides a preparation method for polyurethane gel.

Description

聚氨酯凝胶及其制备方法Polyurethane gel and preparation method thereof
交叉引用cross reference
本申请要求2021年12月14日提交的申请号为2021115282104的中国专利申请的优先权。上述申请的内容以引用方式被包含于此。This application claims the priority of the Chinese Patent Application No. 2021115282104 filed on December 14, 2021. The content of the above application is incorporated herein by reference.
技术领域technical field
本发明涉及聚氨酯技术领域，尤其涉及一种聚氨酯凝胶及其制备方法。The invention relates to the technical field of polyurethane, in particular to a polyurethane gel and a preparation method thereof.
背景技术Background technique
聚氨酯是聚氨基甲酸酯的简称，英文名称为polyurethane，是一种新兴的有机高分子材料，被誉为“第五大塑料”，因其卓越的性能而被广泛应用于国民经济众多领域，产品应用领域涉及轻工、化工、电子、纺织、医疗、建筑、建材、汽车、国防、航天和航空等。Polyurethane is the abbreviation of polyurethane, and its English name is polyurethane. It is an emerging organic polymer material and is known as the "fifth largest plastic". It is widely used in many fields of the national economy because of its excellent performance. The product application fields involve light industry, chemical industry, electronics, textile, medical treatment, construction, building materials, automobile, national defense, aerospace and aviation, etc.
聚氨酯凝胶由于不含有硅氧烷成分，对环境污染较小，混合方便，用于替代传统有机硅凝胶，是一类应用非常广泛的凝胶。Since polyurethane gel does not contain siloxane components, it has less pollution to the environment and is easy to mix. It is used to replace traditional silicone gel and is a type of gel that is widely used.
公开号为CN107848285A的中国专利公开了一种聚氨酯凝胶及其制造方法，聚氨酯凝胶具备凝胶层和被覆所述凝胶层的涂覆层，所述凝胶层是通过至少使平均官能团数超过2.0的脂肪族多异氰酸酯与平均官能团数为3.0以下的多元醇进行反应而得到的，所述涂覆层是通过至少使脂肪族二异氰酸酯及/或脂环族二异氰酸酯与2官能性活性氢化合物进行反应而得到的，通过异氰酸酯与树脂中的羟基进行反应，从而能够降低异氰酸酯的含量，使得聚氨酯凝胶的硬度降低，但当聚氨酯凝胶被使用在发热量大的电子部件中时，由于聚氨酯凝胶散热效果差，热量聚集在聚氨酯凝胶中无法快速散去，容易导致电子部件被烧坏。The Chinese patent with the publication number CN107848285A discloses a polyurethane gel and its manufacturing method. The polyurethane gel has a gel layer and a coating layer covering the gel layer. The gel layer is obtained by at least making the average number of functional groups The coating layer is obtained by reacting an aliphatic polyisocyanate exceeding 2.0 with a polyol having an average functional group number of 3.0 or less, and the coating layer is obtained by at least making aliphatic diisocyanate and/or alicyclic diisocyanate and difunctional active hydrogen It is obtained by reacting the isocyanate and the hydroxyl group in the resin, so that the content of isocyanate can be reduced, so that the hardness of the polyurethane gel is reduced, but when the polyurethane gel is used in electronic components with high heat generation, due to Polyurethane gel has poor heat dissipation effect, and the heat accumulated in polyurethane gel cannot be dissipated quickly, which may easily cause electronic components to be burned out.
因此，有必要开发一种聚氨酯凝胶及其制备方法，以避免现有技术中存在的上述问题。Therefore, it is necessary to develop a polyurethane gel and a preparation method thereof to avoid the above-mentioned problems in the prior art.
发明内容Contents of the invention
本发明的目的在于提供一种聚氨酯凝胶及其制备方法，解决了聚氨酯凝胶无法快速散热，导致电子部件被烧坏的问题，同时得到的聚氨酯凝胶的硬度较低，使得电子部件发生碰撞时，聚氨酯凝胶能起到缓冲效果。The purpose of the present invention is to provide a polyurethane gel and its preparation method, which solves the problem that the polyurethane gel cannot dissipate heat quickly, causing the electronic components to be burned out, and at the same time, the hardness of the obtained polyurethane gel is low, which makes the electronic components collide , polyurethane gel can play a cushioning effect.
为实现上述目的，本发明所述的一种聚氨酯凝胶，包括导热固化剂组分和导热树脂组分；In order to achieve the above object, a polyurethane gel according to the present invention includes a thermally conductive curing agent component and a thermally conductive resin component;
所述导热固化剂组分包括固化剂组分和第一导热填料，所述导热树脂组分包括树脂组分和第二导热填料；The thermally conductive curing agent component includes a curing agent component and a first thermally conductive filler, and the thermally conductive resin component includes a resin component and a second thermally conductive filler;
所述固化剂组分包括羟基树脂和异氰酸酯类扩链剂，所述树脂组分包括催化剂和羟基树脂；The curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the resin component includes a catalyst and a hydroxyl resin;
所述导热固化剂组分和所述导热树脂组分的体积比为1:1。The volume ratio of the thermally conductive curing agent component to the thermally conductive resin component is 1:1.
本发明所述聚氨酯凝胶的有益效果在于：通过所述羟基树脂和所述异氰酸酯类扩链剂进行预聚反应以得到所述固化剂组分，使得所述固化剂组分中的所述异氰酸酯的含量降低，从而使得所述聚氨酯凝胶的硬度较低；所述导热固化剂组分包括固化剂组分和导热填料，所述导热树脂组分包括树脂组分和导热填料，所述固化剂组分和所述树脂组分分别加入导热填料，使得聚氨酯凝胶具有良好的导热效果，从而解决了聚氨酯凝胶无法快速散热，导致电子部件被烧坏的问题，同时得到的聚氨酯凝胶的硬度较低，使得电子部件发生碰撞时，聚氨酯凝胶能够起到缓冲效果。The beneficial effect of the polyurethane gel of the present invention is that: the curing agent component is obtained through the prepolymerization reaction of the hydroxyl resin and the isocyanate chain extender, so that the isocyanate in the curing agent component content is reduced, so that the hardness of the polyurethane gel is lower; the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, the thermally conductive resin component includes a resin component and a thermally conductive filler, and the curing agent The component and the resin component are respectively added with thermally conductive fillers, so that the polyurethane gel has a good thermal conductivity effect, thereby solving the problem that the polyurethane gel cannot dissipate heat quickly and cause the electronic components to be burned out. At the same time, the hardness of the polyurethane gel obtained is Low, so that when the electronic components collide, the polyurethane gel can play a cushioning effect.
可选的，以占所述导热固化剂组分的质量百分比计，所述固化剂组分的含量为8％～20％，所述第一导热填料的含量为80％～92％。Optionally, based on the mass percentage of the thermally conductive curing agent component, the content of the curing agent component is 8% to 20%, and the content of the first thermally conductive filler is 80% to 92%.
可选的，以占所述导热树脂组分的质量百分比计，所述树脂组分的含量为3％～19％，所述第二导热填料的含量为81％～97％。Optionally, based on the mass percentage of the thermally conductive resin component, the content of the resin component is 3%-19%, and the content of the second thermally conductive filler is 81%-97%.
可选的，以占所述固化剂组分的质量百分比计，所述固化剂组分中的所述羟基树脂的含量为60％～90％，所述异氰酸酯类扩链剂的含量为10％～40％。Optionally, based on the mass percentage of the curing agent component, the content of the hydroxyl resin in the curing agent component is 60% to 90%, and the content of the isocyanate chain extender is 10%. ~40%.
可选的，以占所述树脂组分的质量百分比计，所述催化剂的含量为0.1％～1％，所述树脂组分中的所述羟基树脂的含量为99％～99.9％。Optionally, based on the mass percentage of the resin component, the content of the catalyst is 0.1%-1%, and the content of the hydroxyl resin in the resin component is 99%-99.9%.
可选的，所述异氰酸酯类扩链剂为二苯甲烷二异氰酸酯、异佛尔酮二异氰酸酯、多异氰酸酯和六亚甲基二异氰酸酯中的任意一种。Optionally, the isocyanate chain extender is any one of diphenylmethane diisocyanate, isophorone diisocyanate, polyisocyanate and hexamethylene diisocyanate.
可选的，所述固化剂组分中的所述羟基树脂和所述树脂组分中的所述羟基树脂均为聚醚多元醇、聚酯多元醇、蓖麻油、改性蓖麻油和山梨醇中的任意一种。Optionally, the hydroxyl resin in the curing agent component and the hydroxyl resin in the resin component are polyether polyol, polyester polyol, castor oil, modified castor oil and sorbitol any of the.
可选的，所述聚氨酯凝胶的导热系数为1.5W/mK～3.0W/mK。其有益效果在于：使得所述聚氨酯凝胶能够快速散热，从而能够防止电子部件被烧坏。Optionally, the thermal conductivity of the polyurethane gel is 1.5W/mK˜3.0W/mK. The beneficial effect is that the polyurethane gel can quickly dissipate heat, thereby preventing electronic components from being burned out.
可选的，所述催化剂为二月桂酸二丁基锡催化剂、胺类催化剂和有机锌催化剂中的任意一种。其有益效果在于：通过添加催化剂，使得导热固化剂组分和导热树脂组分能够反应更完全，且缩短反应时间。Optionally, the catalyst is any one of dibutyltin dilaurate catalyst, amine catalyst and organozinc catalyst. The beneficial effect is that by adding the catalyst, the heat-conducting curing agent component and the heat-conducting resin component can react more completely, and the reaction time is shortened.
进一步可选的，所述胺类催化剂为脂肪族胺类催化剂、脂环族胺类催化剂、醇类化合物催化剂和芳香族胺类催化剂中的任意一种。Further optionally, the amine catalyst is any one of aliphatic amine catalysts, alicyclic amine catalysts, alcohol compound catalysts and aromatic amine catalysts.
本发明的另一目的在于提供一种聚氨酯凝胶的制备方法，包括以下步骤：Another object of the present invention is to provide a kind of preparation method of polyurethane gel, comprises the following steps:
使用羟基树脂与异氰酸酯类扩链剂进行反应以制得固化剂组分；Use hydroxyl resin to react with isocyanate chain extender to prepare curing agent component;
使用所述固化剂组分与第一导热填料进行混合以制得导热固化剂组分；mixing the curing agent component with the first thermally conductive filler to obtain a thermally conductive curing agent component;
使用催化剂与羟基树脂进行混合以制得树脂组分；Mixing with a hydroxyl resin using a catalyst to produce a resin component;
使用所述树脂组分与第二导热填料进行混合以制得导热树脂组分；mixing the resin component with a second thermally conductive filler to prepare a thermally conductive resin component;
使用所述导热固化剂组分与所述导热树脂组分进行反应以制得所述聚氨酯凝胶，并使所述导热固化剂组分和所述导热树脂组分的体积比为1:1。The heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1.
本发明所述聚氨酯凝胶的制备方法的有益效果在于：所述固化剂组分包括羟基树脂和异氰酸酯类扩链剂，通过所述羟基树脂和所述异氰酸酯类扩链剂进行预聚反应以得到所述固化剂组分，使得所述固化剂组分中的所述异氰酸酯的 含量降低，从而使得所述聚氨酯凝胶的硬度较低；所述导热树脂组分包括催化剂，能够加快后续所述导热树脂组分和所述导热固化剂组分的反应，从而缩短反应时间；所述导热固化剂组分包括固化剂组分和导热填料，所述导热树脂组分包括树脂组分和导热填料，所述固化剂组分和所述树脂组分分别加入导热填料，使得聚氨酯凝胶具有良好的导热效果，从而解决了聚氨酯凝胶无法快速散热，导致电子部件被烧坏的问题，同时得到的聚氨酯凝胶的硬度较低，使得电子部件发生碰撞时，聚氨酯凝胶能够起到缓冲效果。The beneficial effect of the preparation method of the polyurethane gel of the present invention is that: the curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the hydroxyl resin and the isocyanate chain extender are prepolymerized to obtain The curing agent component reduces the content of the isocyanate in the curing agent component, thereby making the hardness of the polyurethane gel lower; the thermally conductive resin component includes a catalyst, which can accelerate the subsequent heat conduction The reaction of the resin component and the thermally conductive curing agent component, thereby shortening the reaction time; the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, and the thermally conductive resin component includes a resin component and a thermally conductive filler, so The above-mentioned curing agent component and the above-mentioned resin component are respectively added with thermally conductive fillers, so that the polyurethane gel has a good thermal conductivity effect, thus solving the problem that the polyurethane gel cannot dissipate heat quickly and cause the electronic components to be burned out. At the same time, the obtained polyurethane gel The hardness of the glue is low, so that when the electronic components collide, the polyurethane gel can play a cushioning effect.
可选的，所述使用羟基树脂与异氰酸酯类扩链剂进行反应以制得固化剂组分的步骤包括：将所述羟基树脂与所述异氰酸酯类扩链剂混合均匀后，进行升温搅拌反应以制得所述固化剂组分。Optionally, the step of using a hydroxyl resin to react with an isocyanate chain extender to prepare a curing agent component includes: after uniformly mixing the hydroxyl resin and the isocyanate chain extender, performing a temperature-raising stirring reaction to Prepare the curing agent component.
可选的，所述升温搅拌反应的温度为25℃～120℃，所述升温搅拌反应的时间为30min～6h。Optionally, the temperature of the heating and stirring reaction is 25° C. to 120° C., and the time of the heating and stirring reaction is 30 minutes to 6 hours.
附图说明Description of drawings 具体实施方式Detailed ways
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。除非另外定义，此处使用的技术术语或者科学术语应当为本发明所属领域内具有一般技能的人士所理解的通常意义。本文中使用的“包括”等类似的词语意指出现该词前面的元件或者物件涵盖出现在该词后面列举的元件或者物件及其等同，而不排除其他元件或者物件。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of them. the embodiment. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention. Unless otherwise defined, the technical terms or scientific terms used herein shall have the usual meanings understood by those skilled in the art to which the present invention belongs. As used herein, "comprising" and similar words mean that the elements or items appearing before the word include the elements or items listed after the word and their equivalents, without excluding other elements or items.
本发明的实施例中，提供了一种聚氨酯凝胶，包括导热固化剂组分和导热树脂组分；In an embodiment of the present invention, a polyurethane gel is provided, including a thermally conductive curing agent component and a thermally conductive resin component;
所述导热固化剂组分包括固化剂组分和第一导热填料，所述导热树脂组分包括树脂组分和第二导热填料；The thermally conductive curing agent component includes a curing agent component and a first thermally conductive filler, and the thermally conductive resin component includes a resin component and a second thermally conductive filler;
所述固化剂组分包括羟基树脂和异氰酸酯类扩链剂，所述树脂组分包括催化剂和羟基树脂；The curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the resin component includes a catalyst and a hydroxyl resin;
所述导热固化剂组分和所述导热树脂组分的体积比为1:1。通过所述羟基树脂和所述异氰酸酯类扩链剂进行预聚反应以得到所述固化剂组分，使得所述固化剂组分中的所述异氰酸酯的含量降低，从而使得所述聚氨酯凝胶的硬度较低；所述导热固化剂组分包括固化剂组分和导热填料，所述导热树脂组分包括树脂组分和导热填料，所述固化剂组分和所述树脂组分分别加入导热填料，使得聚氨酯凝胶具有良好的导热效果，从而解决了聚氨酯凝胶无法快速散热，导致电子部件被烧坏的问题，同时得到的聚氨酯凝胶的硬度较低，使得电子部件发生碰撞时，聚氨酯凝胶能够起到缓冲效果。The volume ratio of the thermally conductive curing agent component to the thermally conductive resin component is 1:1. The curing agent component is obtained by performing a prepolymerization reaction with the hydroxyl resin and the isocyanate chain extender, so that the content of the isocyanate in the curing agent component is reduced, thereby making the polyurethane gel The hardness is low; the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, the thermally conductive resin component includes a resin component and a thermally conductive filler, and the curing agent component and the resin component are respectively added with a thermally conductive filler , so that the polyurethane gel has a good heat conduction effect, thereby solving the problem that the polyurethane gel cannot dissipate heat quickly, causing the electronic components to be burned out. At the same time, the obtained polyurethane gel has a low hardness, so that when the electronic components collide Glue can play a cushioning effect.
本发明的一些实施例中，以占所述导热固化剂组分的质量百分比计，所述固化剂组分的含量为8％～20％，所述第一导热填料的含量为80％～92％。In some embodiments of the present invention, based on the mass percentage of the thermally conductive curing agent component, the content of the curing agent component is 8% to 20%, and the content of the first thermally conductive filler is 80% to 92%. %.
本发明的一些实施例中，以占所述导热树脂组分的质量百分比计，所述树脂组分的含量为3％～19％，所述第二导热填料的含量为81％～97％。In some embodiments of the present invention, based on the mass percentage of the thermally conductive resin component, the content of the resin component is 3%-19%, and the content of the second thermally conductive filler is 81%-97%.
本发明的一些实施例中，以占所述固化剂组分的质量百分比计，所述固化剂组分中的所述羟基树脂的含量为60％～90％，所述异氰酸酯类扩链剂的含量为10％～40％。In some embodiments of the present invention, based on the mass percentage of the curing agent component, the content of the hydroxyl resin in the curing agent component is 60% to 90%, and the content of the isocyanate chain extender is The content is 10% to 40%.
本发明的一些实施例中，以占所述树脂组分的质量百分比计，所述催化剂的含量为0.1％～1％，所述树脂组分中的所述羟基树脂的含量为99％～99.9％。In some embodiments of the present invention, based on the mass percentage of the resin component, the content of the catalyst is 0.1% to 1%, and the content of the hydroxyl resin in the resin component is 99% to 99.9% %.
本发明的一些实施例中，所述异氰酸酯类扩链剂为二苯甲烷二异氰酸酯、异佛尔酮二异氰酸酯、多异氰酸酯和六亚甲基二异氰酸酯中的任意一种。In some embodiments of the present invention, the isocyanate chain extender is any one of diphenylmethane diisocyanate, isophorone diisocyanate, polyisocyanate and hexamethylene diisocyanate.
本发明的一些实施例中，所述固化剂组分中的所述羟基树脂和所述树脂组分中的所述羟基树脂均为聚醚多元醇、聚酯多元醇、蓖麻油、改性蓖麻油和山梨醇中的任意一种。In some embodiments of the present invention, the hydroxyl resin in the curing agent component and the hydroxyl resin in the resin component are polyether polyol, polyester polyol, castor oil, modified castor Either of sesame oil and sorbitol.
本发明的实施例中，所述聚氨酯凝胶的导热系数为1.5W/mK～3.0W/mK。使得所述聚氨酯凝胶能够快速散热，从而能够防止电子部件被烧坏。In an embodiment of the present invention, the thermal conductivity of the polyurethane gel is 1.5W/mK˜3.0W/mK. The polyurethane gel can quickly dissipate heat, thereby preventing electronic components from being burned out.
本发明的一些实施例中，所述催化剂为二月桂酸二丁基锡催化剂、胺类催化剂和有机锌催化剂中的任意一种。通过添加催化剂，使得导热固化剂组分和导热树脂组分能够反应更完全，且缩短反应时间。In some embodiments of the present invention, the catalyst is any one of dibutyltin dilaurate catalyst, amine catalyst and organozinc catalyst. By adding a catalyst, the thermally conductive curing agent component and the thermally conductive resin component can react more completely and shorten the reaction time.
本发明的一些可能实施例中，所述胺类催化剂为脂肪族胺类催化剂、脂环族胺类催化剂、醇类化合物催化剂和芳香族胺类催化剂中的任意一种。In some possible embodiments of the present invention, the amine catalyst is any one of aliphatic amine catalysts, alicyclic amine catalysts, alcohol compound catalysts and aromatic amine catalysts.
本发明的一些可能实施例中，所述脂肪族胺类催化剂为N,N-二甲基环己胺、双(2-二甲氨基乙基)醚、N,N,N',N'-四甲基亚烷基二胺、三乙胺和N,N-二甲基苄胺中的任意一种。In some possible embodiments of the present invention, the aliphatic amine catalyst is N,N-dimethylcyclohexylamine, bis(2-dimethylaminoethyl)ether, N,N,N',N'- Any one of tetramethylalkylenediamine, triethylamine and N,N-dimethylbenzylamine.
本发明的一些可能实施例中，所述脂环族胺类催化剂为固胺、N-乙基吗啉、N,N-二甲基甲酰胺(NMM)和N,N’-二乙基哌嗪中的任意一种。In some possible embodiments of the present invention, the cycloaliphatic amine catalyst is solid amine, N-ethylmorpholine, N,N-dimethylformamide (NMM) and N,N'-diethylpiper any of the oxazines.
本发明的一些可能实施例中，所述醇类化合物催化剂为三乙醇胺和二甲基乙醇胺(DMEA)中的任意一种。In some possible embodiments of the present invention, the alcohol compound catalyst is any one of triethanolamine and dimethylethanolamine (DMEA).
本发明的再一些具体实施例中，所述芳香族胺类催化剂为吡啶和N,N’-二甲基吡啶中的任意一种。In still some specific embodiments of the present invention, the aromatic amine catalyst is any one of pyridine and N,N'-lutidine.
本发明的一些可能实施例中，所述催化剂为N,N-二甲基环己胺、双(2-二甲氨基乙基)醚、N,N,N',N'-四甲基亚烷基二胺、三乙胺、N,N-二甲基苄胺、固胺、N-乙基吗啉、N,N-二甲基甲酰胺(NMM)、N,N’-二乙基哌嗪、三乙醇胺、二甲基乙醇胺(DMEA)、吡啶和N,N’-二甲基吡啶中的任意一种。In some possible embodiments of the present invention, the catalyst is N,N-dimethylcyclohexylamine, bis(2-dimethylaminoethyl)ether, N,N,N',N'-tetramethylethylene Alkyldiamine, triethylamine, N,N-dimethylbenzylamine, solid amine, N-ethylmorpholine, N,N-dimethylformamide (NMM), N,N'-diethyl Any one of piperazine, triethanolamine, dimethylethanolamine (DMEA), pyridine and N,N'-lutidine.
本发明的实施例中，提供了一种聚氨酯凝胶的制备方法，包括以下步骤：In the embodiment of the present invention, a kind of preparation method of polyurethane gel is provided, comprising the following steps:
使用羟基树脂与异氰酸酯类扩链剂进行反应以制得固化剂组分；Use hydroxyl resin to react with isocyanate chain extender to prepare curing agent component;
使用所述固化剂组分与第一导热填料进行混合以制得导热固化剂组分；mixing the curing agent component with the first thermally conductive filler to obtain a thermally conductive curing agent component;
使用催化剂与羟基树脂进行混合以制得树脂组分；Mixing with a hydroxyl resin using a catalyst to produce a resin component;
使用所述树脂组分与第二导热填料进行混合以制得导热树脂组分；mixing the resin component with a second thermally conductive filler to prepare a thermally conductive resin component;
使用所述导热固化剂组分与所述导热树脂组分进行反应以制得所述聚氨酯凝胶，并使所述导热固化剂组分和所述导热树脂组分的体积比为1:1。所述固化剂组分包括羟基树脂和异氰酸酯类扩链剂，通过所述羟基树脂和所述异氰酸酯类扩链剂进行预聚反应以得到所述固化剂组分，使得所述固化剂组分中的所述异氰酸酯的含量降低，从而使得所述聚氨酯凝胶的硬度较低；所述导热树脂组分包括催化剂，能够加快后续所述导热树脂组分和所述导热固化剂组分的反应，从而缩短反应时间；所述导热固化剂组分包括固化剂组分和导热填料，所述导热树脂组分包括树脂组分和导热填料，所述固化剂组分和所述树脂组分分别加入导热填料，使得聚氨酯凝胶具有良好的导热效果，从而解决了聚氨酯凝胶无法快速散热，导致电子部件被烧坏的问题，同时得到的聚氨酯凝胶的硬度较低，使得电子部件发生碰撞时，聚氨酯凝胶能够起到缓冲效果。The heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1. The curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the curing agent component is obtained by performing a prepolymerization reaction between the hydroxyl resin and the isocyanate chain extender, so that in the curing agent component The content of the isocyanate is reduced, so that the hardness of the polyurethane gel is lower; the thermally conductive resin component includes a catalyst, which can accelerate the subsequent reaction of the thermally conductive resin component and the thermally conductive curing agent component, thereby Shorten the reaction time; the thermally conductive curing agent component includes a curing agent component and a thermally conductive filler, the thermally conductive resin component includes a resin component and a thermally conductive filler, and the curing agent component and the resin component are respectively added with a thermally conductive filler , so that the polyurethane gel has a good heat conduction effect, thereby solving the problem that the polyurethane gel cannot dissipate heat quickly, causing the electronic components to be burned out. At the same time, the obtained polyurethane gel has a low hardness, so that when the electronic components collide Glue can play a cushioning effect.
本发明的一些实施例中，所述使用羟基树脂与异氰酸酯类扩链剂进行反应以制得固化剂组分的步骤包括：将所述羟基树脂与所述异氰酸酯类扩链剂混合均匀后，进行升温搅拌反应以制得所述固化剂组分。In some embodiments of the present invention, the step of using a hydroxyl resin to react with an isocyanate chain extender to prepare a curing agent component includes: after uniformly mixing the hydroxyl resin and the isocyanate chain extender, performing The temperature is raised and the reaction is stirred to obtain the curing agent component.
本发明的一些实施例中，所述升温搅拌反应的温度为25℃～120℃，所述升温搅拌反应的时间为30min～6h。In some embodiments of the present invention, the temperature of the heating and stirring reaction is 25° C. to 120° C., and the time of the heating and stirring reaction is 30 minutes to 6 hours.
本发明的一些实施例中，所述导热填料包括导热粉体和偶联剂。In some embodiments of the present invention, the thermally conductive filler includes thermally conductive powder and a coupling agent.
本发明的一些实施例中，所述导热粉体包括氢氧化铝、氧化铝、氮化硼和 氮化铝中的至少一种。In some embodiments of the present invention, the thermally conductive powder includes at least one of aluminum hydroxide, aluminum oxide, boron nitride and aluminum nitride.
本发明的另一些实施例中，所述导热填料的制备方法，包括以下步骤：In other embodiments of the present invention, the preparation method of the thermally conductive filler includes the following steps:
称量导热粉体放置于高速分散机中，对导热粉体进行分散；将偶联剂添加至分散机里分散0.5h-3h以制备导热填料；其中所述偶联剂和所述导热粉体的质量比为(0.001～0.01):1。Weigh the thermally conductive powder and place it in a high-speed disperser to disperse the thermally conductive powder; add a coupling agent to the disperser and disperse for 0.5h-3h to prepare a thermally conductive filler; wherein the coupling agent and the thermally conductive powder The mass ratio is (0.001～0.01):1.
实施例1-8和对比例Embodiment 1-8 and comparative example
本发明的实施例1-8和对比例分别提供了一种聚氨酯凝胶，其具体组成和含量见表1。实施例1-8与对比例的区别在于：实施例1-8中聚氨酯凝胶中的成分包括导热填料，对比例中的聚氨酯凝胶中的成分不包括导热填料。Examples 1-8 and comparative examples of the present invention respectively provide a polyurethane gel, and its specific composition and content are shown in Table 1. The difference between Examples 1-8 and Comparative Example is that the components in the polyurethane gel in Examples 1-8 include thermally conductive fillers, and the components in the polyurethane gel in Comparative Examples do not include thermally conductive fillers.
表1 实施例1-8和对比例的组成和含量The composition and content of table 1 embodiment 1-8 and comparative example
Figure PCTCN2022113451-appb-000001
Figure PCTCN2022113451-appb-000001
Figure PCTCN2022113451-appb-000002
Figure PCTCN2022113451-appb-000002
实施例1～8的制备方法如下：The preparation method of embodiment 1～8 is as follows:
将所述羟基树脂与所述异氰酸酯类扩链剂混合均匀后，在温度为25℃～120℃的条件下反应30min～6h，以制得所述固化剂组分；After uniformly mixing the hydroxyl resin and the isocyanate chain extender, react at a temperature of 25° C. to 120° C. for 30 minutes to 6 hours to obtain the curing agent component;
使用所述固化剂组分与第一导热填料进行混合以制得导热固化剂组分；mixing the curing agent component with the first thermally conductive filler to obtain a thermally conductive curing agent component;
使用催化剂与羟基树脂进行混合以制得树脂组分；Mixing with a hydroxyl resin using a catalyst to produce a resin component;
使用所述树脂组分与第二导热填料进行混合以制得导热树脂组分；mixing the resin component with a second thermally conductive filler to prepare a thermally conductive resin component;
使用所述导热固化剂组分与所述导热树脂组分进行反应以制得所述聚氨酯凝胶，并使所述导热固化剂组分和所述导热树脂组分的体积比为1:1。The heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1.
对比例的制备方法如下：The preparation method of comparative example is as follows:
将所述羟基树脂与所述异氰酸酯类扩链剂混合均匀后，在温度为25℃～120℃的条件下反应30min～6h，以制得所述固化剂组分；After uniformly mixing the hydroxyl resin and the isocyanate chain extender, react at a temperature of 25° C. to 120° C. for 30 minutes to 6 hours to obtain the curing agent component;
使用催化剂与羟基树脂进行混合以制得树脂组分；Mixing with a hydroxyl resin using a catalyst to produce a resin component;
使用所述固化剂组分与所述树脂组分进行反应以制得所述聚氨酯凝胶，并使所述固化剂组分和所述树脂组分的体积比为1:1。The curing agent component is used to react with the resin component to prepare the polyurethane gel, and the volume ratio of the curing agent component to the resin component is 1:1.
性能评估：Performance evaluation:
使用标准ASTM D5470中的试验方法测试导热系数；使用标准ASTM D2240中的试验方法测试硬度。Thermal conductivity was tested using the test method in standard ASTM D5470; hardness was tested using the test method in standard ASTM D2240.
对实施例1～8得到的所述聚氨酯凝胶的导热系数和硬度进行测试，测试结果 见表2。The thermal conductivity and the hardness of the polyurethane gel obtained in Examples 1-8 are tested, and the test results are shown in Table 2.
表2 所述聚氨酯凝胶的性能参数The performance parameter of polyurethane gel described in table 2
Figure PCTCN2022113451-appb-000003
Figure PCTCN2022113451-appb-000003
从表2中可知，本发明中聚氨酯凝胶的导热系数为2.0W/mK～2.3W/mK，而对比例中聚氨酯凝胶的导热系数为0.3W/mK，本发明中聚氨酯凝胶的导热系数远大于对比例中聚氨酯凝胶的导热系数；本发明中聚氨酯凝胶的硬度为OO56度～OO75度，而对比例中聚氨酯凝胶的硬度为OO20度，本发明中聚氨酯凝胶的硬度远大于对比例中聚氨酯凝胶的硬度，对比例中聚氨酯凝胶的缓冲效果优于本发明中聚氨酯凝胶的缓冲效果，但是本发明的聚氨酯凝胶也符合市场对硬度的要求。As can be seen from Table 2, the thermal conductivity of the polyurethane gel in the present invention is 2.0W/mK～2.3W/mK, while the thermal conductivity of the polyurethane gel in the comparative example is 0.3W/mK, the thermal conductivity of the polyurethane gel in the present invention The coefficient is far greater than the thermal conductivity of the polyurethane gel in the comparative example; the hardness of the polyurethane gel in the present invention is 0056 degree to 0075 degree, and the hardness of the polyurethane gel in the comparative example is 0020 degree, and the hardness of the polyurethane gel in the present invention is much larger Regarding the hardness of the polyurethane gel in the comparative example, the cushioning effect of the polyurethane gel in the comparative example is better than that of the polyurethane gel in the present invention, but the polyurethane gel of the present invention also meets the market's requirements for hardness.
前述的实例仅是说明性的，用于解释本发明所述方法的一些特征。所附的权利要求旨在要求可以设想的尽可能广的范围，且本文所呈现的实施例仅是根据所有可能的实施例的组合的选择的实施方式的说明。因此，申请人的用意是所附的权利要求不被说明本发明的特征的示例的选择限制。在权利要求中所用的一些数值范围也包括了在其之内的子范围，这些范围中的变化也应在可能的情况下解释为被所附的权利要求覆盖。The foregoing examples are illustrative only, and are used to explain some features of the methods described in the present invention. The appended claims are intended to claim the broadest scope conceivable and the embodiments presented herein are merely illustrations of selected implementations according to all possible combinations of embodiments. Accordingly, it is the applicant's intention that the appended claims not be limited by the selection of examples which characterize the invention. Certain numerical ranges used in the claims also include sub-ranges therein, and changes within these ranges should also be construed as being covered by the appended claims where possible.

Claims (13)

  1. 一种聚氨酯凝胶，其特征在于，包括导热固化剂组分和导热树脂组分；A polyurethane gel, characterized in that it includes a thermally conductive curing agent component and a thermally conductive resin component;
    所述导热固化剂组分包括固化剂组分和第一导热填料，所述导热树脂组分包括树脂组分和第二导热填料；The thermally conductive curing agent component includes a curing agent component and a first thermally conductive filler, and the thermally conductive resin component includes a resin component and a second thermally conductive filler;
    所述固化剂组分包括羟基树脂和异氰酸酯类扩链剂，所述树脂组分包括催化剂和羟基树脂；The curing agent component includes a hydroxyl resin and an isocyanate chain extender, and the resin component includes a catalyst and a hydroxyl resin;
    所述导热固化剂组分和所述导热树脂组分的体积比为1:1。The volume ratio of the thermally conductive curing agent component to the thermally conductive resin component is 1:1.
  2. 根据权利要求1所述的聚氨酯凝胶，其特征在于，以占所述导热固化剂组分的质量百分比计，所述固化剂组分的含量为8％～20％，所述第一导热填料的含量为80％～92％。The polyurethane gel according to claim 1, characterized in that, based on the mass percentage of the thermally conductive curing agent component, the content of the curing agent component is 8% to 20%, and the first thermally conductive filler The content is 80% to 92%.
  3. 根据权利要求1所述的聚氨酯凝胶，其特征在于，以占所述导热树脂组分的质量百分比计，所述树脂组分的含量为3％～19％，所述第二导热填料的含量为81％～97％。The polyurethane gel according to claim 1, characterized in that, based on the mass percentage of the thermally conductive resin component, the content of the resin component is 3% to 19%, and the content of the second thermally conductive filler 81% to 97%.
  4. 根据权利要求1所述的聚氨酯凝胶，其特征在于，以占所述固化剂组分的质量百分比计，所述固化剂组分中的所述羟基树脂的含量为60％～90％，所述异氰酸酯类扩链剂的含量为10％～40％。The polyurethane gel according to claim 1, characterized in that, based on the mass percentage of the curing agent component, the content of the hydroxyl resin in the curing agent component is 60% to 90%, so The content of the isocyanate chain extender is 10%-40%.
  5. 根据权利要求1所述的聚氨酯凝胶，其特征在于，以占所述树脂组分的质量百分比计，所述催化剂的含量为0.1％～1％，所述树脂组分中的所述羟基树脂的含量为99％～99.9％。The polyurethane gel according to claim 1, characterized in that, based on the mass percentage of the resin component, the content of the catalyst is 0.1% to 1%, and the hydroxyl resin in the resin component is The content is 99% to 99.9%.
  6. 根据权利要求1所述的聚氨酯凝胶，其特征在于，所述异氰酸酯类扩链剂为二苯甲烷二异氰酸酯、异佛尔酮二异氰酸酯、多异氰酸酯和六亚甲基二异氰酸酯中的任意一种。The polyurethane gel according to claim 1, wherein the isocyanate chain extender is any one of diphenylmethane diisocyanate, isophorone diisocyanate, polyisocyanate and hexamethylene diisocyanate .
  7. 根据权利要求1所述的聚氨酯凝胶，其特征在于，所述固化剂组分中的 所述羟基树脂和所述树脂组分中的所述羟基树脂均为聚醚多元醇、聚酯多元醇、蓖麻油、改性蓖麻油和山梨醇中的任意一种。The polyurethane gel according to claim 1, characterized in that, the hydroxyl resin in the curing agent component and the hydroxyl resin in the resin component are polyether polyol, polyester polyol , castor oil, modified castor oil and sorbitol any one.
  8. 根据权利要求1所述的聚氨酯凝胶，其特征在于，所述聚氨酯凝胶的导热系数为1.5W/mK～3.0W/mK。The polyurethane gel according to claim 1, characterized in that the thermal conductivity of the polyurethane gel is 1.5W/mK˜3.0W/mK.
  9. 根据权利要求1所述的聚氨酯凝胶，其特征在于，所述催化剂为二月桂酸二丁基锡催化剂、胺类催化剂和有机锌催化剂中的任意一种。The polyurethane gel according to claim 1, wherein the catalyst is any one of a dibutyltin dilaurate catalyst, an amine catalyst and an organozinc catalyst.
  10. 根据权利要求9所述的聚氨酯凝胶，其特征在于，所述胺类催化剂为脂肪族胺类催化剂、脂环族胺类催化剂、醇类化合物催化剂和芳香族胺类催化剂中的任意一种。The polyurethane gel according to claim 9, wherein the amine catalyst is any one of aliphatic amine catalysts, alicyclic amine catalysts, alcohol compound catalysts and aromatic amine catalysts.
  11. 一种聚氨酯凝胶的制备方法，其特征在于，包括以下步骤：A preparation method of polyurethane gel, is characterized in that, comprises the following steps:
    使用羟基树脂与异氰酸酯类扩链剂进行反应以制得固化剂组分；Use hydroxyl resin to react with isocyanate chain extender to prepare curing agent component;
    使用所述固化剂组分与第一导热填料进行混合以制得导热固化剂组分；mixing the curing agent component with the first thermally conductive filler to obtain a thermally conductive curing agent component;
    使用催化剂与羟基树脂进行混合以制得树脂组分；Mixing with a hydroxyl resin using a catalyst to produce a resin component;
    使用所述树脂组分与第二导热填料进行混合以制得导热树脂组分；mixing the resin component with a second thermally conductive filler to prepare a thermally conductive resin component;
    使用所述导热固化剂组分与所述导热树脂组分进行反应以制得所述聚氨酯凝胶，并使所述导热固化剂组分和所述导热树脂组分的体积比为1:1。The heat-conducting curing agent component is used to react with the heat-conducting resin component to prepare the polyurethane gel, and the volume ratio of the heat-conducting curing agent component and the heat-conducting resin component is 1:1.
  12. 根据权利要求11所述的聚氨酯凝胶的制备方法，其特征在于，所述使用羟基树脂与异氰酸酯类扩链剂进行反应以制得固化剂组分的步骤包括：The preparation method of polyurethane gel according to claim 11, characterized in that, the step of using a hydroxyl resin to react with an isocyanate chain extender to obtain a curing agent component comprises:
    将所述羟基树脂与所述异氰酸酯类扩链剂混合均匀后，进行升温搅拌反应以制得所述固化剂组分。After the hydroxyl resin and the isocyanate chain extender are uniformly mixed, they are stirred and reacted at elevated temperature to obtain the curing agent component.
  13. 根据权利要求12所述的聚氨酯凝胶的制备方法，其特征在于，所述升温搅拌反应的温度为25℃～120℃，所述升温搅拌反应的时间为30min～6h。The preparation method of polyurethane gel according to claim 12, characterized in that, the temperature of the heating and stirring reaction is 25° C. to 120° C., and the time of the heating and stirring reaction is 30 minutes to 6 hours.
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CN113736419A (en) * 2021-10-19 2021-12-03 杭州之江新材料有限公司 Double-component polyurethane heat-conducting structural adhesive and preparation method thereof

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